Concentration of mica



Patented Dec. 1, 1942 CONCENTRATION OF MICA Francis X. Tartar-on andAllen T. Cole, Mulberry,

Fla, assignors to Phosphate Recovery Corporation, New York, N. Y., acorporation of Delaware No Drawing.

9 Claims.

This invention relates to a froth-flotation process for theconcentration of mica from mixtures containing mica and impurities suchas clay, feldspar, quartz and silicious material. The general object ofthe invention is to produce a clean, bright,' mica concentratecontaining negligible clay or grit and having a weight per cubic footacceptable to the trade. Such weight of mica concentrates is usuallyrequired by the trade to be less than 20 lbs. per cubic foot; and thisis attained by the use of the invention hereinafter described.

The usual fatty acids and their soaps when used alone have been found tobe ineffective for the concentration of mica by froth-flotation of themica. Tartaron and Harrison, assignors to the same assignee to which thepresent application is assigned, it is pointed out that an alkaliresinate such as sodium resinate is an effective agent for theconcentration of mica by froth-flotation.

The processes for concentrating mica hereinafter described are theresult of several discoveries. One -of these discoveries is that by theuse of certain inorganic compounds which act as activating agents, notonly are improved results obtained when an alkali resinate such assodium resinate is employed as the flotation agent as described in saidTartaron and Harrison patent, but also that other anionic collectors aremade effective for the froth-flotation of mica. These activating agentsare salts and bases of the alkaline earth metals, including calcium,barium, magnesium and strontium, and their compounds includinghydroxides, carbonates, chlorides, etc. Capable of employment inconjunction with these activators are anionic collectors such as fattyacids, resin acids, naphthenic acids, tall oils and their soaps.Frothers such as pine oil or pine tar oils such as P. T. 101 may also beof assistance in concentrating mica by froth-flotation with the useof'the activating agents and flotation agents which have been mentioned.

We have also discovered that pre-agitation of the mica ore pulp withwater prior to addition of reagents efiects improved results. Our beliefis that this may be due to the breaking up of books Application May 21,1941, Serial No. 394,498

' treated in the same manner if desired.

In U. S. Patent No. 2,226,103 to The following examples illustrate theprocess of the present invention. The material treated was a micaceousproduct derived from the washer of Kaolin, Inc., at Spruce Pine, N. C.The mica present was muscovite intermixed with clay, feldspar, quartzand silicious material. The examples merely illustrate the processes ofthe in vention and are not to be construed as limiting its scope. Allcubic weight figures are in pounds per cubic foot.

Examples 1 and 2 are comparative and show the beneficial effect ofemploying lime as an activator in connection with an alkali resinatesuch as sodium resinate.

Example 1.No activator.A charge of micaceous material, known as sand boxpaper clay derived from Kaolin, Inc., was placed in a frothiiotationmachine and diluted to form a pulp of about 10% solids. To this pulp wasadded sodium resinate in the amount of 5 lbs. per ton of solids in thepulp, and pine oil in the-amount of 0.42' lb. per ton of such solids.After brief agitation in the froth-flotation machine a rougher froth wasproduced; and this rougher froth was diluted with water and a cleanerfroth-float was made therefrom without any further addition of agents.Tailings of this second operation were considered middlings which wouldbe returned to the rougher flotation machine. The results were asfollows:

of prod.

Example 2.With lime as an activator.The operations of Example 1 wererepeated, except that 1.5 lbs. of lime per ton of solids in the feedwere added to the pulp which was then subjected to brief agitation,after which the sodium resinate .and pine oil were added in the samequantities as in Example 1, and the thus conditioned pulp was subjectedto the same treatments as in the case of Example 1. The were as follows:

It will be noted that while the recovery in Example 2 is somewhat lessthan in Example 1 thegrade of mica concentrate was improved from 19.00lbs. to 14.13 lbs. per cubic foot. Thus it is obvious that the use withsodium resinate of lime as an activator gives highly beneficial results.

The following Examples "3 and 4 illustrate the beneficial effect ofpre-agitation of the ore pulp with water. before addition of theactivating and flotation agents. These tests were made on another sampleof fsand box settlings also obtained from Kaolin, Inc.

Example 3.No pre-agitation with water.-A charge of "sand box settlingsalso obtained from Kaolin, Inc. was placed in a froth-floation machineas a pulp at about 40% solids. To this charge was added 2.5 lbs. of limeper ton of solids in the feed, after which the pulp was subjected tobrief agitation; and then there were added 6.0 lbs. of sodium resinateand 0.42 lb. of pine 011, both per ton of solids in the feed. and thepulp was again subjected to brief agitation. After diluting thisconditioned pulp to about 10% solids, a rougher froth-float wasproduced. This rougher frothfloat was returned to the flotation machine,and to it were added 0.4 lb. of lime and 0.14 lb. of pine oil, both perton of solids in the original feed; and after dilution a cleanerfroth-float was made. This cleaner froth-float was also returned to themachine, and to it were added 0.3 lb. of lime and 0.14 lb. of pine oil.both per ton of solids in the original feed; and after suitable dilutiona recleaner froth-float. was produced. The results were as follows:

Percent Products wt.of

feed

Feed 100.0 ma (lone 28.9 11.4 Mlds-2 111 22.9 Mids-I 10.4 25.1 Tails I54.0 31.0

Example 4.Pre-agitation with water.--The treatments in this example wereidentical with Example 3, except that the ore pulp at about 40% solidswas agitated for aboutlo minutes in the froth-flotation machine prior tothe initial or first addition of the lime. The results were as follows:

Per cent cm wt Products g of prod.

rm! 100.0 20. 3 Com 30. 6 16.8 Mids-2 M 25.1 Mids-l 1o. 9 2a 1 ails. as.1 32.1

It will be apparent that the recovery in Example 4 was slightly betterthan in Example 3; and that the grade of mica concentrate was improvedfrom 17.4 lbs. to 15.8 lbs. per cubic foot; thereby proving thatpre-agitation of the mica or pulp before adding the agents wasbeneficial.

The following Examples 5, 6 and 7 illustrate the'successful use ofvarious fatty acids in conjunction with lime, in froth-flotationconcentration of mica.- In these examples, the amount of lime was 2.5lbs. and the amount of. pine oil was 0.28 lbs. both per ton of solids inthe feed. In

. each example the material treated was sand box .settlings obtainedfrom Kaolin, Inc.

Example 5.--A pulp containing the material to be treated in the amountof about 500 g. at 40% solids was agitated in a laboratory flotationmachine for about 10 minutes. Then the lime was added and the pulp wasagain briefly agitated. To the pulp was then added 4.03 lbs. of Upjohn'sfatty acid (an animal fatty acid) per ton of solids in the original feedtogether with the pine oil;

after which the pulp was again briefly agitated.

After diluting the thus conditioned pulp to about 10% solids, a rougherfroth-float was produced and removed. This rougher froth was returned tothe machine, 0.40 lb. of lime per ton of solids in the originalfeed wasadded, and after suitable dilution a cleaner froth-float was made. Thiscleaner froth was also returned to the machine, treated with 0.30 lb. oflime per ton of solids in the original feed, diluted and a final micafrothfloat was made. The results were as follows:

Per cent Cu. wt

Products wtegi prod Feed 100. 0 26. 8 Cone 24. 9 l5. 5 Mids-2 5. 7 24. 5Mids-l 12.8 as 2 Tails 66. 0 29.0

Conc.+Midse2 30. 6 17. 2

Example 6. 'Ihe treatments in this example were identical with Example5, except that 4.99 lbs. of red oil (crude oleic acid) was used insteadof Upjohn's fatty acid. The results were as follows:

Per cent Cubic Product wt. of wt. of

feed prod.

Feed 100. 0 20. 3 Cone l8. 5 l5. 1 Mills-2 5. 3 22. 4 Mids-l 12. 8 20. 0Tails I 03. 4 a0. 0 Cono.+Mid-2 at 1111 Example 7..The treatments inthis example were identical with Examples 5 and 6, except that, as thefatty acid, 3.07 lbs. of Chatham fatty acid was used. This fatty acid isa tall 011- or paper mill by-product containing resin acids andvegetable fatty acids. The results were as fol- It will be noted that ineach of Examples 5, 6 and 7 a mica concentrate was produced the weightof which was considerably below 20 lbs. per cubic foot; therebyprovingthat various fatty acids,

when used in conjunction with lime as an activator, result insatisfactory concentration of mice. by froth-flotation.

The following Examples 8, 9, 10 and 11 illustrate the successful usewith a fatty acid of the activating agents, of the kind hereinbeforementioned, such as calcium chloride, magnesium carbonate, bariumhydroidde and strontium hydroxide. In each of these examples, Chathamfatty acid to the amount of 3.07 lbs. and pine oil in the amount of 0.28lb., both per ton of solids in the feed, were employed. The materialtreated was again sand box settlings obtained from Kaolin, Inc.

Example 8.A charge of about 500 g. of the material to be treated wasagitated in a flotation machine for about 10 minutes at 40% solids. Then8.75 lbs. of calcium chloride per ton of solids in the pulp was added,after which the pulp was again briefly agitated. Then the Chatham fattyacid and pine oil were added and the pulp was conditioned. The pulp wasthen diluted to about 10% sollds'and a mica frothfloat was made andremoved. The results were as follows:

Example 9.-In this treatment, the activator was magnesium carbonate inthe amount of 2.85 lbs. per ton of solids in the pulp which was brieflyagitated prior to the addition of the fatty acid and pine oil with whichthe pulp was then conditioned. The thus conditioned pulp was sub- Jectedto froth-flotation and a rougher mica froth-float was removed. Thisrougher froth was subjected to a cleaner froth-flotation treatment afterthe addition to it of 0.46 lb. of magnesium carbonate per ton of solidsin the original feed; and the froth-float thus obtained was subjected tore-cleaner froth-flotation treatment after the addition of 0.34 lb. ofmagnesium carbonate per ton of solids in the orignal feed. The resultsof these operations were as follows:

Per cent Cubic wt. Pmdu'ct wt. oifeed of prod.

100. 26. 3 2i. 9 l5. 8 8. 7 23.9 19. l 29. 3 50. 3 30. l

Conc.+Mids-2 30. 6 18. 1

Example 10.The treatments in this example were the same as in Example 9,except that the activator used was barium hydroxide to the amount of5.78 lbs. in the rougher treatment, 0.93 lb. in the cleaner treatmentand 0.67 lb. in the re-cleaner treatment, all per ton of solids in theoriginal feed. The results were as follows:

Example 11.-The treatments in this example were the same as in Example9, except that the activator was strontium hydroxide which was added tothe amounts of 6.64 lbs. in the rougher treatment, 4.26 lbs. in thecleaner treatment, and 3.19 lbs. in the re-cleaner treatment, all perton of solids in the original feed. The results were as follows:

Per cent Cubic wt. I wt. oileed oi prod.

Feed 100. 0 26. 3 Cone 27. 8 l6. 9 5. 4 22. 9 ll. 4 30. 6 55. 4 30. 5

Conc.+Mids-2 33. 2 l7. 9

Example 12.'-In this treatment, as in Example 9, the activator wasmagnesium carbonate, but

the flotation agent was sodium resinate which Per cent Cubic Product wt.of wt. oi

teed prod.

Feed .L 100.0 25.3 Conc.. 22. 7 l6. 4 MldS-Z--- 4.6 22.1 Mids-l--- 7.727.4 I ails cs0 30.8

Conc.+Mids-2 27. 3 l7. 3

The following Examples 13 and 14 show successful concentration of micaby froth-flotation of the mica by the use, with lime as an activatingagent, of sodium oleate or naphthenic acid. As before, the mica materialtreated was sand box settlings obtained from Kaolin, Inc.

Example 13.-An aqueous pulp of the mica ore was agitated in afroth-flotation machine for about ten minutes at 40% solids, diluted to10% solids; and then again briefly agitated with lime to the amount of3.80 lbs. per ton of solids in the feed. To this pulp were added 6.00lbs.

of sodium oleate and 0.42 lb. of pine oil, both per ton of solids in thefeed, and the pulp was then subjected to brief agitation. The thusconditioned pulp was subjected to froth-flotation and a rougher micafroth-float was removed. This rougherfroth after being reconditionedwith 0.70 lb. of lime and 0.28 lb. of

- pine oil, both per ton of solids in the original feed. was subjectedto froth-flotation to produce the final mica concentrate in thefroth-float. The results were as follows:

Per cent Cubic Product wt. of wt. of

feed prod Conc.+Mids 36. 6 19. 3

Example 14.-An adueous pulp of the mica ore was agitated in a.froth-flotation machine for about ten minutes at 40% solids; and thenlime, to the amount of 2.50 lbs. per ton of solids in the feed, wasadded and the pulp was again briefly agitated. To this thick pulp wereadded naphthenic acid to the amount of 6.00 lbs., pine oil to the amountof 0.42 11)., both per ton of solids in the feed, and the pulp was thenagitated for about two minutes. After dilution to solids, the thusconditioned pulp was subjected to froth-flotation and arougherfrothfloat was removed. This rougher froth, after reconditioningwith 0.40 lb. of lime and 0.28 lb. of pine oil, both per ton'of solidsin the ori inal feed, was subjected to froth-flotation and a firstcleaner froth-float was removed; and this cleaner froth-float, .atterreconditioning with 0.30 lb. of lime and 0.28 lb. of pine 011, both perton of solids in the original feed, was subjected' to froth-flotation toproduce 'the final concentrate. The results were as follows:

From the foregoing Examples 8 to 14 inclusive, it will be apparent thatthe activators hereinbefore mentioned, of which lime, calcium chloride,magnesium carbonate, barium hydroxide and strontium hydroxide areexamples, permit the' use of fatty acids, naphthenic acids, resin acidsand their soaps in the froth-flotation concentration of mica.

-silicious material,

What is claimed is:

1. The process for the concentration of mica from a mixture of mica withimpurities 'comprising principally clay, feldspar, quartz and comprisingadding to an aqueous pulp of such .micaceous mixture a reagentconsisting of an' inorganic compound of an alkaline earth .metal servingas an activator for .the mica together with an anionic collector, andseparating the mica from said mixture by froth-flotation of the micaaway from the other ingredients of-the mixture.

2. The-process of claiml, in which the aqueous pulp is agitated prior tothe addition of reagents.

Q 3. The pl Qcss of claim 1, in which the inorganic compound is selectedfrom the class consisting of oxides and hydroxides of alkaline earthmetals. 4

4. The process of cla 1', in which the inorganic compound is lime.-

5. The process of claim 1. in whi'chthe inorganic compound ismagnesiumcarbonate.

6. The process ofclaim '1, in which'the'inorganic compound is bariumhydroxide.

7. The process of claim 1; in which'the'a'nionic collector-is selectedfrom the group consisting of fatty acids, resin acids, oils and theirsoaps.

- 8. The process of claim 1, in which a frother is employed inconjunction with the activator andcollecton-v- 9. The process of claim1, in which the reagents are added in tion treatments.

naphthenic acids, tall more x TARTARON. mm '1'. com.

steps to a plurality of dots-- CERTIFICATE; OF combmmn; Patent 110.2,505,962. December 1', 19!;2.

mncxs x. mnmnom', ET AL.

.It is hereby oertitied'that error appeara-i'in'the prgitedspecification of the above numbered patent requiriqg correction astfolloyva: Page 1,flr'et column, line 21, after Broth-flotation andbefore the period insert--01 the mica-:; page 1 .tfiretf' oolunih, line10, "after *rougher' insert -"-m1ca lines 18- and 1-9, for "finalconcentrate read final mica concentrate in thefroth-floht-q and that thesaid. Letters Patent shoplq be readwith t i correctiqn thereip that thesame IhB-Y conform to the record or the case 1n ,the Patent Office.

Signed a sealer} this 19th day of January, A, n. 191;

(Seell' --He nry Van Arsdale, v

- .Aeting Commissioner of Patents.

